# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_Cambridge 0222
#TrackingRef 'Compound1_CCDC759030_k09132.cif'
_publ_contact_author_name 'Gino G. Lavoie'
_publ_contact_author_address
;Department of Chemistry
York University
4700 Keele Street
Toronto, Ontario
Canada, M3J 1P3
;
_publ_contact_author_email glavoie@yorku.ca
_publ_contact_author_phone +1-416-736-2100
_publ_contact_author_fax +1-416-736-5936
loop_
_publ_author_name
_publ_author_address
G.G.Lavoie
;Department of Chemistry
York University
4700 Keele Street
Toronto, Ontario
Canada, M3J 1P3
;
A.C.Badaj
;Department of Chemistry
York University
4700 Keele Street
Toronto, Ontario
Canada, M3J 1P3
;
S.Dastgir
;Department of Chemistry
York University
4700 Keele Street
Toronto, Ontario
Canada, M3J 1P3
;
A.Lough
;Department of Chemistry
University of Toronto
80 St. George Street
Toronto, Ontario
Canada, M5S 3H6
;
data_k09132
_database_code_depnum_ccdc_archive 'CCDC 759030'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C22 H26 N3, C H2 Cl2, Cl'
_chemical_formula_sum 'C23 H28 Cl3 N3'
_chemical_formula_weight 452.83
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 9.0219(2)
_cell_length_b 26.6329(7)
_cell_length_c 10.7548(3)
_cell_angle_alpha 90.00
_cell_angle_beta 113.6980(14)
_cell_angle_gamma 90.00
_cell_volume 2366.25(10)
_cell_formula_units_Z 4
_cell_measurement_temperature 150(1)
_cell_measurement_reflns_used 20220
_cell_measurement_theta_min 2.6
_cell_measurement_theta_max 25.0
_exptl_crystal_description needle
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.12
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.271
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 952
_exptl_absorpt_coefficient_mu 0.401
# Absorption correction
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.475
_exptl_absorpt_correction_T_max 0.955
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_measurement_method '\f scans and \w scans with \k offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 20220
_diffrn_reflns_av_R_equivalents 0.1302
_diffrn_reflns_av_sigmaI/netI 0.0816
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -31
_diffrn_reflns_limit_k_max 31
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_theta_min 2.57
_diffrn_reflns_theta_max 25.00
_reflns_number_total 4151
_reflns_number_gt 2676
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'Collect (Nonius B.V., 1997-2002)'
_computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction Denzo-SMN
_computing_structure_solution 'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_molecular_graphics 'PLATON (Spek, 2003)'
_computing_publication_material 'SHELXTL V6.1'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A.,
Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst.
27, 435.
Blessing, R. H. (1995). Acta Cryst. A51, 33-38.
Nonius B.V (1997-2002). Collect. Data collection software, Delft,
The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
Macromolecular Crystallography, Part A edited by C. W. Carter &
R. M. Sweet pp. 307-326. London: Academic press.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13.
;
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+2.1629P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 4151
_refine_ls_number_parameters 268
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1043
_refine_ls_R_factor_gt 0.0582
_refine_ls_wR_factor_ref 0.1799
_refine_ls_wR_factor_gt 0.1383
_refine_ls_goodness_of_fit_ref 1.076
_refine_ls_restrained_S_all 1.076
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.39661(11) 0.49022(3) 0.69142(9) 0.0364(3) Uani 1 1 d . . .
N1 N 0.1479(3) 0.54180(10) 0.3147(3) 0.0300(7) Uani 1 1 d . . .
N2 N 0.1637(3) 0.46261(10) 0.3587(3) 0.0283(7) Uani 1 1 d . . .
N3 N 0.1287(3) 0.38165(10) 0.4094(3) 0.0328(7) Uani 1 1 d . . .
C1 C 0.2445(4) 0.50226(12) 0.3414(4) 0.0290(8) Uani 1 1 d . . .
H1A H 0.3524 0.5020 0.3473 0.035 Uiso 1 1 calc R . .
C2 C 0.0090(4) 0.47756(13) 0.3417(4) 0.0302(8) Uani 1 1 d . . .
H2A H -0.0734 0.4569 0.3483 0.036 Uiso 1 1 calc R . .
C3 C -0.0009(4) 0.52699(13) 0.3142(4) 0.0318(8) Uani 1 1 d . . .
H3A H -0.0921 0.5480 0.2976 0.038 Uiso 1 1 calc R . .
C4 C 0.2271(4) 0.41234(12) 0.3950(3) 0.0280(8) Uani 1 1 d . . .
C5 C 0.3964(4) 0.40480(13) 0.4108(4) 0.0362(9) Uani 1 1 d . . .
H5A H 0.4229 0.3690 0.4227 0.054 Uiso 1 1 calc R . .
H5B H 0.4696 0.4234 0.4905 0.054 Uiso 1 1 calc R . .
H5C H 0.4087 0.4171 0.3296 0.054 Uiso 1 1 calc R . .
C6 C 0.1747(4) 0.33026(12) 0.4417(4) 0.0323(9) Uani 1 1 d . . .
C7 C 0.2602(4) 0.31569(13) 0.5768(4) 0.0360(9) Uani 1 1 d . . .
C8 C 0.2930(5) 0.26432(14) 0.6007(5) 0.0463(11) Uani 1 1 d . . .
H8A H 0.3521 0.2531 0.6911 0.056 Uiso 1 1 calc R . .
C9 C 0.2418(5) 0.22968(14) 0.4967(4) 0.0451(10) Uani 1 1 d . . .
H9A H 0.2673 0.1951 0.5156 0.054 Uiso 1 1 calc R . .
C10 C 0.1532(5) 0.24532(14) 0.3651(4) 0.0420(10) Uani 1 1 d . . .
H10A H 0.1164 0.2212 0.2940 0.050 Uiso 1 1 calc R . .
C11 C 0.1170(4) 0.29583(13) 0.3351(4) 0.0360(9) Uani 1 1 d . . .
C12 C 0.3132(5) 0.35276(15) 0.6923(4) 0.0503(11) Uani 1 1 d . . .
H12A H 0.3762 0.3796 0.6744 0.075 Uiso 1 1 calc R . .
H12B H 0.3802 0.3356 0.7769 0.075 Uiso 1 1 calc R . .
H12C H 0.2177 0.3672 0.7008 0.075 Uiso 1 1 calc R . .
C13 C 0.0160(5) 0.31344(16) 0.1931(4) 0.0504(11) Uani 1 1 d . . .
H13A H -0.0753 0.3333 0.1932 0.076 Uiso 1 1 calc R . .
H13B H -0.0249 0.2843 0.1333 0.076 Uiso 1 1 calc R . .
H13C H 0.0825 0.3342 0.1601 0.076 Uiso 1 1 calc R . .
C14 C 0.1867(4) 0.59198(12) 0.2841(4) 0.0299(8) Uani 1 1 d . . .
C15 C 0.1989(4) 0.60005(13) 0.1609(4) 0.0321(8) Uani 1 1 d . . .
C16 C 0.2322(4) 0.64865(13) 0.1330(4) 0.0351(9) Uani 1 1 d . . .
H16A H 0.2423 0.6552 0.0499 0.042 Uiso 1 1 calc R . .
C17 C 0.2510(4) 0.68807(13) 0.2228(4) 0.0354(9) Uani 1 1 d . . .
C18 C 0.2405(4) 0.67765(13) 0.3461(4) 0.0360(9) Uani 1 1 d . . .
H18A H 0.2556 0.7042 0.4091 0.043 Uiso 1 1 calc R . .
C19 C 0.2086(4) 0.62951(12) 0.3797(4) 0.0304(8) Uani 1 1 d . . .
C20 C 0.1793(5) 0.55826(14) 0.0602(4) 0.0407(10) Uani 1 1 d . . .
H20A H 0.0881 0.5368 0.0536 0.061 Uiso 1 1 calc R . .
H20B H 0.2785 0.5381 0.0909 0.061 Uiso 1 1 calc R . .
H20C H 0.1585 0.5727 -0.0290 0.061 Uiso 1 1 calc R . .
C21 C 0.2783(5) 0.74091(14) 0.1860(4) 0.0458(10) Uani 1 1 d . . .
H21A H 0.3332 0.7605 0.2691 0.069 Uiso 1 1 calc R . .
H21B H 0.1739 0.7565 0.1313 0.069 Uiso 1 1 calc R . .
H21C H 0.3456 0.7401 0.1337 0.069 Uiso 1 1 calc R . .
C22 C 0.2004(5) 0.61973(14) 0.5142(4) 0.0383(9) Uani 1 1 d . . .
H22A H 0.2535 0.6472 0.5769 0.057 Uiso 1 1 calc R . .
H22B H 0.2554 0.5880 0.5517 0.057 Uiso 1 1 calc R . .
H22C H 0.0869 0.6175 0.5019 0.057 Uiso 1 1 calc R . .
Cl2 Cl 0.24227(13) 0.41884(4) 0.01073(12) 0.0543(3) Uani 1 1 d . . .
Cl3 Cl 0.56487(13) 0.37525(4) 0.10681(12) 0.0542(3) Uani 1 1 d . . .
C23 C 0.4441(5) 0.42834(14) 0.0303(4) 0.0455(10) Uani 1 1 d . . .
H23A H 0.4889 0.4583 0.0874 0.055 Uiso 1 1 calc R . .
H23B H 0.4465 0.4344 -0.0597 0.055 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0347(5) 0.0341(5) 0.0416(6) -0.0017(4) 0.0167(4) -0.0025(4)
N1 0.0308(16) 0.0220(15) 0.0358(18) 0.0028(13) 0.0120(14) 0.0009(12)
N2 0.0294(16) 0.0255(15) 0.0293(17) 0.0017(12) 0.0109(13) 0.0003(12)
N3 0.0320(16) 0.0261(15) 0.0421(19) 0.0045(13) 0.0168(15) -0.0003(13)
C1 0.0302(19) 0.0244(18) 0.033(2) 0.0019(15) 0.0132(17) -0.0002(15)
C2 0.0270(19) 0.0289(19) 0.037(2) 0.0039(15) 0.0148(16) 0.0005(15)
C3 0.0276(19) 0.034(2) 0.038(2) 0.0032(17) 0.0177(17) 0.0033(15)
C4 0.0294(18) 0.0246(18) 0.029(2) 0.0009(14) 0.0107(16) 0.0021(15)
C5 0.034(2) 0.0276(19) 0.050(2) 0.0062(17) 0.0197(18) 0.0045(16)
C6 0.0277(19) 0.0261(18) 0.046(2) 0.0059(17) 0.0176(17) 0.0022(15)
C7 0.040(2) 0.0268(19) 0.044(2) 0.0037(17) 0.0201(18) -0.0012(16)
C8 0.044(2) 0.034(2) 0.056(3) 0.012(2) 0.015(2) 0.0077(18)
C9 0.051(2) 0.0218(19) 0.065(3) 0.0067(19) 0.026(2) 0.0053(18)
C10 0.048(2) 0.029(2) 0.053(3) -0.0044(18) 0.025(2) -0.0028(17)
C11 0.036(2) 0.032(2) 0.043(2) -0.0005(17) 0.0187(18) 0.0022(16)
C12 0.060(3) 0.038(2) 0.044(3) 0.0023(19) 0.012(2) 0.000(2)
C13 0.053(3) 0.046(2) 0.047(3) -0.005(2) 0.015(2) 0.000(2)
C14 0.0264(18) 0.0240(18) 0.037(2) 0.0058(16) 0.0099(16) 0.0035(14)
C15 0.0315(19) 0.0291(19) 0.034(2) 0.0021(16) 0.0108(17) 0.0034(15)
C16 0.037(2) 0.032(2) 0.035(2) 0.0075(17) 0.0132(17) 0.0016(16)
C17 0.037(2) 0.0237(18) 0.043(2) 0.0048(16) 0.0139(18) 0.0015(15)
C18 0.039(2) 0.0278(19) 0.040(2) -0.0007(17) 0.0153(18) 0.0059(16)
C19 0.0315(19) 0.0286(19) 0.032(2) 0.0022(15) 0.0132(16) 0.0041(15)
C20 0.049(2) 0.034(2) 0.039(2) -0.0016(18) 0.0170(19) -0.0042(18)
C21 0.056(3) 0.031(2) 0.049(3) 0.0052(18) 0.019(2) -0.0006(18)
C22 0.045(2) 0.033(2) 0.041(2) 0.0038(17) 0.0219(19) 0.0035(17)
Cl2 0.0482(6) 0.0474(6) 0.0625(8) 0.0056(5) 0.0172(6) 0.0054(5)
Cl3 0.0525(7) 0.0549(7) 0.0569(8) 0.0027(5) 0.0237(6) 0.0105(5)
C23 0.053(3) 0.038(2) 0.047(3) -0.0024(19) 0.022(2) -0.0078(19)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.323(4) . ?
N1 C3 1.398(4) . ?
N1 C14 1.452(4) . ?
N2 C1 1.338(4) . ?
N2 C2 1.391(4) . ?
N2 C4 1.447(4) . ?
N3 C4 1.262(4) . ?
N3 C6 1.432(4) . ?
C2 C3 1.344(5) . ?
C4 C5 1.480(5) . ?
C6 C11 1.395(5) . ?
C6 C7 1.399(5) . ?
C7 C8 1.402(5) . ?
C7 C12 1.506(5) . ?
C8 C9 1.378(6) . ?
C9 C10 1.381(6) . ?
C10 C11 1.391(5) . ?
C11 C13 1.505(5) . ?
C14 C15 1.389(5) . ?
C14 C19 1.390(5) . ?
C15 C16 1.389(5) . ?
C15 C20 1.513(5) . ?
C16 C17 1.390(5) . ?
C17 C18 1.395(5) . ?
C17 C21 1.509(5) . ?
C18 C19 1.393(5) . ?
C19 C22 1.501(5) . ?
Cl2 C23 1.765(4) . ?
Cl3 C23 1.773(4) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C3 108.9(3) . . ?
C1 N1 C14 125.8(3) . . ?
C3 N1 C14 125.3(3) . . ?
C1 N2 C2 109.3(3) . . ?
C1 N2 C4 126.1(3) . . ?
C2 N2 C4 124.6(3) . . ?
C4 N3 C6 120.0(3) . . ?
N1 C1 N2 108.1(3) . . ?
C3 C2 N2 106.5(3) . . ?
C2 C3 N1 107.3(3) . . ?
N3 C4 N2 114.3(3) . . ?
N3 C4 C5 130.0(3) . . ?
N2 C4 C5 115.8(3) . . ?
C11 C6 C7 122.6(3) . . ?
C11 C6 N3 116.9(3) . . ?
C7 C6 N3 120.2(3) . . ?
C6 C7 C8 116.7(4) . . ?
C6 C7 C12 122.3(3) . . ?
C8 C7 C12 121.0(4) . . ?
C9 C8 C7 121.8(4) . . ?
C8 C9 C10 119.8(3) . . ?
C9 C10 C11 121.0(4) . . ?
C10 C11 C6 118.0(4) . . ?
C10 C11 C13 121.8(4) . . ?
C6 C11 C13 120.2(3) . . ?
C15 C14 C19 123.5(3) . . ?
C15 C14 N1 118.5(3) . . ?
C19 C14 N1 118.0(3) . . ?
C16 C15 C14 117.2(3) . . ?
C16 C15 C20 120.3(3) . . ?
C14 C15 C20 122.5(3) . . ?
C15 C16 C17 122.0(4) . . ?
C16 C17 C18 118.3(3) . . ?
C16 C17 C21 120.6(3) . . ?
C18 C17 C21 121.0(3) . . ?
C19 C18 C17 122.0(3) . . ?
C14 C19 C18 116.9(3) . . ?
C14 C19 C22 122.7(3) . . ?
C18 C19 C22 120.3(3) . . ?
Cl2 C23 Cl3 110.7(2) . . ?
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 0.334
_refine_diff_density_min -0.422
_refine_diff_density_rms 0.081
_vrf_PLAT061_k09132
;
PROBLEM: Tmax/Tmin Range Test RR' too Large ............. 0.54
RESPONSE: ...
This Alert is generated when the predicted transmission coefficients
are different from the calculated ones. Since the multi-scan correction
uses redundant data it corrects for more than just absorption: slight
crystal alignment, poor crystal quality and maybe even sometimes
partial twinning. When there are many kappa data sets within one
collection, I have found the transmission factors appear larger than
they should and this is sometimes to do with inter-set scaling. You
would expect this Alert to appear more for low absorbers (organics)
where the absorption is minimal but the multi-scan absorption
correction has been used.
;
# end Validation Reply Form
# Attachment 'Compound2_CCDC759031_k09165.cif'
data_k09165
_database_code_depnum_ccdc_archive 'CCDC 759031'
#TrackingRef 'Compound2_CCDC759031_k09165.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C22 H25 Ag Cl N3, C H2 Cl2'
_chemical_formula_sum 'C23 H27 Ag Cl3 N3'
_chemical_formula_weight 559.70
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_H-M 'P 21 21 21'
_symmetry_space_group_name_Hall 'P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
_cell_length_a 9.1037(2)
_cell_length_b 15.7675(3)
_cell_length_c 17.1993(3)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 2468.83(8)
_cell_formula_units_Z 4
_cell_measurement_temperature 150(1)
_cell_measurement_reflns_used 22758
_cell_measurement_theta_min 2.6
_cell_measurement_theta_max 27.5
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.26
_exptl_crystal_size_min 0.22
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.506
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1136
_exptl_absorpt_coefficient_mu 1.156
# Absorption correction
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.724
_exptl_absorpt_correction_T_max 0.773
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_measurement_method '\f scans and \w scans with \k offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number 22758
_diffrn_reflns_av_R_equivalents 0.0371
_diffrn_reflns_av_sigmaI/netI 0.0352
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_theta_min 2.58
_diffrn_reflns_theta_max 27.49
_reflns_number_total 5650
_reflns_number_gt 5039
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'Collect (Nonius B.V., 1997-2002)'
_computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction Denzo-SMN
_computing_structure_solution 'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_molecular_graphics 'PLATON (Spek, 2003)'
_computing_publication_material 'SHELXTL V6.1'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A.,
Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst.
27, 435.
Blessing, R. H. (1995). Acta Cryst. A51, 33-38.
Nonius B.V (1997-2002). Collect. Data collection software, Delft,
The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
Macromolecular Crystallography, Part A edited by C. W. Carter &
R. M. Sweet pp. 307-326. London: Academic press.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13.
;
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+2.0815P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.08(3)
_refine_ls_number_reflns 5650
_refine_ls_number_parameters 305
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.0439
_refine_ls_R_factor_gt 0.0349
_refine_ls_wR_factor_ref 0.0824
_refine_ls_wR_factor_gt 0.0770
_refine_ls_goodness_of_fit_ref 1.075
_refine_ls_restrained_S_all 1.074
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.63483(3) 0.805138(15) 0.655015(14) 0.02929(8) Uani 1 1 d . . .
Cl1 Cl 0.67508(10) 0.94736(5) 0.62386(5) 0.0347(2) Uani 1 1 d . . .
N1 N 0.5688(3) 0.64071(18) 0.74484(16) 0.0272(6) Uani 1 1 d . . .
N2 N 0.5953(3) 0.61173(18) 0.62421(17) 0.0298(7) Uani 1 1 d . . .
N3 N 0.5628(4) 0.76624(19) 0.81325(17) 0.0304(6) Uani 1 1 d . . .
C1 C 0.5998(4) 0.6770(2) 0.67506(19) 0.0279(7) Uani 1 1 d . . .
C2 C 0.5604(4) 0.5358(2) 0.6617(2) 0.0322(8) Uani 1 1 d . . .
H2A H 0.5499 0.4816 0.6380 0.039 Uiso 1 1 calc R . .
C3 C 0.5448(4) 0.5537(2) 0.7366(2) 0.0327(8) Uani 1 1 d . . .
H3A H 0.5217 0.5147 0.7769 0.039 Uiso 1 1 calc R . .
C4 C 0.5647(4) 0.6863(2) 0.81728(18) 0.0271(7) Uani 1 1 d . . .
C5 C 0.5653(5) 0.6313(2) 0.8882(2) 0.0376(9) Uani 1 1 d . . .
H5A H 0.5698 0.6671 0.9348 0.056 Uiso 1 1 calc R . .
H5B H 0.6510 0.5938 0.8869 0.056 Uiso 1 1 calc R . .
H5C H 0.4754 0.5972 0.8895 0.056 Uiso 1 1 calc R . .
C6 C 0.5616(4) 0.8167(2) 0.88208(19) 0.0304(8) Uani 1 1 d . . .
C7 C 0.4349(5) 0.8244(2) 0.9271(2) 0.0345(8) Uani 1 1 d . . .
C8 C 0.4397(5) 0.8803(3) 0.9907(2) 0.0395(9) Uani 1 1 d . . .
H8A H 0.3550 0.8867 1.0224 0.047 Uiso 1 1 calc R . .
C9 C 0.5651(5) 0.9261(2) 1.0080(2) 0.0415(10) Uani 1 1 d . . .
H9A H 0.5657 0.9634 1.0513 0.050 Uiso 1 1 calc R . .
C10 C 0.6891(5) 0.9180(2) 0.9627(2) 0.0388(9) Uani 1 1 d . . .
H10A H 0.7748 0.9495 0.9750 0.047 Uiso 1 1 calc R . .
C11 C 0.6893(5) 0.8633(2) 0.8983(2) 0.0355(9) Uani 1 1 d . . .
C12 C 0.2954(5) 0.7787(3) 0.9079(2) 0.0438(10) Uani 1 1 d . . .
H12A H 0.2917 0.7676 0.8518 0.066 Uiso 1 1 calc R . .
H12B H 0.2112 0.8137 0.9229 0.066 Uiso 1 1 calc R . .
H12C H 0.2922 0.7248 0.9362 0.066 Uiso 1 1 calc R . .
C13 C 0.8251(5) 0.8538(3) 0.8488(3) 0.0544(11) Uani 1 1 d . . .
H13A H 0.8013 0.8675 0.7947 0.082 Uiso 1 1 calc R . .
H13B H 0.8608 0.7953 0.8519 0.082 Uiso 1 1 calc R . .
H13C H 0.9014 0.8925 0.8676 0.082 Uiso 1 1 calc R . .
C14 C 0.6207(4) 0.6195(2) 0.54100(18) 0.0283(7) Uani 1 1 d . . .
C15 C 0.5120(4) 0.6544(2) 0.4946(2) 0.0315(8) Uani 1 1 d . . .
C16 C 0.5409(5) 0.6602(3) 0.4147(2) 0.0359(9) Uani 1 1 d . . .
H16A H 0.4696 0.6854 0.3817 0.043 Uiso 1 1 calc R . .
C17 C 0.6697(5) 0.6304(3) 0.3826(2) 0.0387(10) Uani 1 1 d . . .
C18 C 0.7756(5) 0.5959(3) 0.4313(2) 0.0368(9) Uani 1 1 d . . .
H18A H 0.8652 0.5761 0.4096 0.044 Uiso 1 1 calc R . .
C19 C 0.7536(4) 0.5895(2) 0.5111(2) 0.0335(8) Uani 1 1 d . . .
C20 C 0.3668(4) 0.6820(2) 0.5269(2) 0.0361(8) Uani 1 1 d . . .
H20A H 0.3825 0.7131 0.5755 0.054 Uiso 1 1 calc R . .
H20B H 0.3057 0.6320 0.5370 0.054 Uiso 1 1 calc R . .
H20C H 0.3173 0.7189 0.4892 0.054 Uiso 1 1 calc R . .
C21 C 0.6995(6) 0.6387(4) 0.2963(2) 0.0610(14) Uani 1 1 d . . .
H21A H 0.6131 0.6630 0.2705 0.091 Uiso 1 1 calc R . .
H21B H 0.7202 0.5826 0.2744 0.091 Uiso 1 1 calc R . .
H21C H 0.7843 0.6759 0.2881 0.091 Uiso 1 1 calc R . .
C22 C 0.8713(5) 0.5530(3) 0.5627(2) 0.0473(10) Uani 1 1 d . . .
H22A H 0.9647 0.5516 0.5344 0.071 Uiso 1 1 calc R . .
H22B H 0.8439 0.4953 0.5781 0.071 Uiso 1 1 calc R . .
H22C H 0.8819 0.5885 0.6092 0.071 Uiso 1 1 calc R . .
Cl2 Cl 0.5759(8) 0.3720(5) 0.2835(4) 0.0744(19) Uani 0.530(19) 1 d PD A 1
Cl3 Cl 0.3205(11) 0.3577(9) 0.2078(6) 0.106(3) Uani 0.530(19) 1 d PD A 1
C24 C 0.4180(13) 0.4293(13) 0.2642(14) 0.109(11) Uani 0.530(19) 1 d PD A 1
H24A H 0.4399 0.4820 0.2352 0.131 Uiso 0.530(19) 1 calc PR A 1
H24B H 0.3644 0.4437 0.3126 0.131 Uiso 0.530(19) 1 calc PR A 1
Cl2A Cl 0.5866(8) 0.4140(13) 0.2846(4) 0.112(4) Uani 0.470(19) 1 d PD A 2
Cl3A Cl 0.3131(7) 0.3969(7) 0.1969(4) 0.071(2) Uani 0.470(19) 1 d PD A 2
C24A C 0.3968(9) 0.4106(15) 0.2865(8) 0.053(4) Uani 0.470(19) 1 d PD A 2
H24C H 0.3603 0.4641 0.3097 0.064 Uiso 0.470(19) 1 calc PR A 2
H24D H 0.3661 0.3636 0.3211 0.064 Uiso 0.470(19) 1 calc PR A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ag1 0.03455(14) 0.02570(12) 0.02762(12) -0.00014(11) 0.00158(12) -0.00311(12)
Cl1 0.0404(5) 0.0268(4) 0.0368(4) 0.0004(3) 0.0056(4) -0.0028(4)
N1 0.0357(17) 0.0239(14) 0.0222(14) 0.0016(11) -0.0009(13) -0.0032(13)
N2 0.0364(18) 0.0277(14) 0.0253(13) -0.0045(11) 0.0061(12) -0.0067(13)
N3 0.0349(17) 0.0330(16) 0.0232(13) -0.0025(12) 0.0010(13) -0.0025(13)
C1 0.0283(18) 0.0298(17) 0.0258(16) -0.0023(12) -0.0007(13) -0.0009(14)
C2 0.041(2) 0.0239(16) 0.0313(17) 0.0018(15) -0.0030(17) -0.0074(15)
C3 0.043(2) 0.0261(17) 0.0293(18) 0.0005(14) -0.0034(16) -0.0050(17)
C4 0.0274(17) 0.0315(18) 0.0225(14) -0.0035(14) -0.0021(13) -0.0022(16)
C5 0.055(3) 0.0323(19) 0.0253(18) 0.0014(15) -0.0060(17) -0.0016(18)
C6 0.042(2) 0.0270(17) 0.0222(15) 0.0006(14) 0.0000(15) 0.0001(16)
C7 0.042(2) 0.037(2) 0.0241(16) 0.0033(14) -0.0007(15) -0.0026(17)
C8 0.057(3) 0.040(2) 0.0216(17) 0.0009(15) 0.0048(17) 0.008(2)
C9 0.071(3) 0.0321(19) 0.0208(17) -0.0017(15) -0.0056(18) 0.000(2)
C10 0.051(2) 0.0308(19) 0.035(2) 0.0002(16) -0.0087(18) -0.0011(18)
C11 0.044(2) 0.0331(19) 0.0296(18) -0.0005(15) -0.0035(17) -0.0017(17)
C12 0.046(2) 0.051(2) 0.034(2) -0.0005(18) 0.0050(18) -0.0050(19)
C13 0.048(3) 0.061(3) 0.054(3) -0.014(2) 0.002(2) -0.014(2)
C14 0.037(2) 0.0274(15) 0.0208(15) -0.0053(12) -0.0004(16) -0.0062(16)
C15 0.035(2) 0.0297(18) 0.0303(18) -0.0010(15) -0.0028(16) -0.0025(16)
C16 0.038(2) 0.041(2) 0.0290(18) 0.0013(16) -0.0041(16) -0.0025(17)
C17 0.043(3) 0.047(2) 0.0263(18) -0.0027(16) 0.0036(17) -0.0050(18)
C18 0.036(2) 0.041(2) 0.0337(19) -0.0071(17) 0.0058(17) -0.0016(18)
C19 0.035(2) 0.0318(19) 0.0333(19) -0.0036(15) 0.0001(16) 0.0010(16)
C20 0.0337(18) 0.044(2) 0.0305(16) -0.0029(15) -0.0035(17) 0.004(2)
C21 0.062(3) 0.090(4) 0.030(2) 0.005(2) 0.009(2) -0.003(3)
C22 0.044(2) 0.057(2) 0.040(2) 0.0018(18) -0.003(2) 0.010(2)
Cl2 0.047(3) 0.112(4) 0.064(2) 0.000(2) -0.0155(18) 0.033(3)
Cl3 0.083(4) 0.135(6) 0.100(4) -0.034(4) -0.012(3) -0.037(4)
C24 0.071(11) 0.15(2) 0.111(16) -0.073(16) 0.020(10) 0.024(11)
Cl2A 0.050(3) 0.234(11) 0.053(2) -0.025(5) 0.0064(17) -0.044(5)
Cl3A 0.037(2) 0.127(6) 0.049(2) -0.009(3) -0.0105(13) 0.005(3)
C24A 0.025(6) 0.098(10) 0.036(5) -0.019(6) 0.001(5) 0.006(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 C1 2.074(3) . ?
Ag1 Cl1 2.3346(9) . ?
N1 C1 1.359(4) . ?
N1 C3 1.397(5) . ?
N1 C4 1.439(4) . ?
N2 C1 1.352(4) . ?
N2 C2 1.397(4) . ?
N2 C14 1.455(4) . ?
N3 C4 1.263(5) . ?
N3 C6 1.426(4) . ?
C2 C3 1.327(5) . ?
C4 C5 1.497(5) . ?
C6 C7 1.395(5) . ?
C6 C11 1.403(5) . ?
C7 C8 1.404(5) . ?
C7 C12 1.497(6) . ?
C8 C9 1.383(6) . ?
C9 C10 1.378(6) . ?
C10 C11 1.403(5) . ?
C11 C13 1.509(6) . ?
C14 C15 1.385(5) . ?
C14 C19 1.397(5) . ?
C15 C16 1.402(5) . ?
C15 C20 1.499(6) . ?
C16 C17 1.378(6) . ?
C17 C18 1.388(6) . ?
C17 C21 1.516(5) . ?
C18 C19 1.390(5) . ?
C19 C22 1.506(6) . ?
Cl2 C24 1.731(8) . ?
Cl3 C24 1.733(8) . ?
Cl2A C24A 1.729(8) . ?
Cl3A C24A 1.733(8) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ag1 Cl1 176.29(9) . . ?
C1 N1 C3 110.9(3) . . ?
C1 N1 C4 124.0(3) . . ?
C3 N1 C4 125.1(3) . . ?
C1 N2 C2 111.2(3) . . ?
C1 N2 C14 124.6(3) . . ?
C2 N2 C14 124.2(3) . . ?
C4 N3 C6 120.7(3) . . ?
N2 C1 N1 104.1(3) . . ?
N2 C1 Ag1 129.7(2) . . ?
N1 C1 Ag1 126.1(2) . . ?
C3 C2 N2 106.8(3) . . ?
C2 C3 N1 106.9(3) . . ?
N3 C4 N1 116.8(3) . . ?
N3 C4 C5 128.5(3) . . ?
N1 C4 C5 114.7(3) . . ?
C7 C6 C11 121.9(3) . . ?
C7 C6 N3 121.1(3) . . ?
C11 C6 N3 116.8(3) . . ?
C6 C7 C8 117.5(4) . . ?
C6 C7 C12 122.4(3) . . ?
C8 C7 C12 120.1(4) . . ?
C9 C8 C7 121.4(4) . . ?
C10 C9 C8 120.4(3) . . ?
C9 C10 C11 120.3(4) . . ?
C10 C11 C6 118.5(4) . . ?
C10 C11 C13 120.5(4) . . ?
C6 C11 C13 121.0(3) . . ?
C15 C14 C19 122.7(3) . . ?
C15 C14 N2 119.2(3) . . ?
C19 C14 N2 118.1(3) . . ?
C14 C15 C16 117.2(4) . . ?
C14 C15 C20 122.1(3) . . ?
C16 C15 C20 120.6(4) . . ?
C17 C16 C15 121.9(4) . . ?
C16 C17 C18 118.9(3) . . ?
C16 C17 C21 121.0(4) . . ?
C18 C17 C21 120.1(4) . . ?
C17 C18 C19 121.6(4) . . ?
C18 C19 C14 117.6(4) . . ?
C18 C19 C22 120.4(4) . . ?
C14 C19 C22 121.9(3) . . ?
Cl2 C24 Cl3 101.1(11) . . ?
Cl2A C24A Cl3A 115.2(8) . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 27.49
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 1.169
_refine_diff_density_min -0.560
_refine_diff_density_rms 0.076
# Attachment 'Compound3_CCDC759032_k09221.cif'
data_k09221
_database_code_depnum_ccdc_archive 'CCDC 759032'
#TrackingRef 'Compound3_CCDC759032_k09221.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C44 H50 Cl Cu N6, 3(C H2 Cl2)'
_chemical_formula_sum 'C47 H56 Cl7 Cu N6'
_chemical_formula_weight 1016.67
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.1810(3)
_cell_length_b 11.2363(3)
_cell_length_c 24.0984(9)
_cell_angle_alpha 98.178(2)
_cell_angle_beta 90.697(2)
_cell_angle_gamma 116.143(2)
_cell_volume 2680.63(14)
_cell_formula_units_Z 2
_cell_measurement_temperature 150(1)
_cell_measurement_reflns_used 28842
_cell_measurement_theta_min 2.6
_cell_measurement_theta_max 27.5
_exptl_crystal_description needle
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.18
_exptl_crystal_size_min 0.14
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.260
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1056
_exptl_absorpt_coefficient_mu 0.792
# Absorption correction
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.566
_exptl_absorpt_correction_T_max 0.695
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 150(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_measurement_method '\f scans and \w scans with \k offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number 24919
_diffrn_reflns_av_R_equivalents 0.063
_diffrn_reflns_av_sigmaI/netI 0.052
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_theta_min 2.55
_diffrn_reflns_theta_max 25.00
_reflns_number_total 9381
_reflns_number_gt 7053
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'Collect (Nonius B.V., 1997-2002)'
_computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction Denzo-SMN
_computing_structure_solution 'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_molecular_graphics 'PLATON (Spek, 2009)'
_computing_publication_material 'SHELXTL V6.1'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A.,
Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst.
27, 435.
Blessing, R. H. (1995). Acta Cryst. A51, 33-38.
Nonius B.V (1997-2002). Collect. Data collection software, Delft,
The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
Macromolecular Crystallography, Part A edited by C. W. Carter &
R. M. Sweet pp. 307-326. London: Academic press.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2009). Acta Cryst. D65, 148--155.
;
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0997P)^2^+1.5560P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 9381
_refine_ls_number_parameters 561
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0775
_refine_ls_R_factor_gt 0.0582
_refine_ls_wR_factor_ref 0.1759
_refine_ls_wR_factor_gt 0.1631
_refine_ls_goodness_of_fit_ref 1.082
_refine_ls_restrained_S_all 1.082
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.75548(4) 0.48580(4) 0.249535(18) 0.02842(15) Uani 1 1 d . . .
Cl1 Cl 0.89521(9) 0.37230(9) 0.22872(5) 0.0434(3) Uani 1 1 d . . .
N1 N 0.5115(3) 0.3404(3) 0.17468(12) 0.0277(6) Uani 1 1 d . . .
N2 N 0.4864(3) 0.2397(3) 0.24553(12) 0.0268(6) Uani 1 1 d . . .
N3 N 0.4007(3) 0.0996(3) 0.30984(12) 0.0305(7) Uani 1 1 d . . .
N4 N 0.9245(3) 0.7090(3) 0.33692(12) 0.0303(7) Uani 1 1 d . . .
N5 N 0.9905(3) 0.7634(3) 0.25717(12) 0.0268(6) Uani 1 1 d . . .
N6 N 1.1075(3) 0.8631(3) 0.18642(13) 0.0334(7) Uani 1 1 d . . .
C1 C 0.5746(3) 0.3514(3) 0.22463(15) 0.0263(7) Uani 1 1 d . . .
C2 C 0.3735(3) 0.1625(3) 0.20760(15) 0.0320(8) Uani 1 1 d . . .
H2A H 0.2996 0.0809 0.2126 0.038 Uiso 1 1 calc R . .
C3 C 0.3892(3) 0.2249(3) 0.16341(16) 0.0331(8) Uani 1 1 d . . .
H3A H 0.3292 0.1966 0.1306 0.040 Uiso 1 1 calc R . .
C4 C 0.5608(3) 0.4326(3) 0.13509(15) 0.0289(8) Uani 1 1 d . . .
C5 C 0.6212(3) 0.3992(4) 0.08901(15) 0.0324(8) Uani 1 1 d . . .
C6 C 0.6620(4) 0.4854(4) 0.04966(16) 0.0395(9) Uani 1 1 d . . .
H6A H 0.7022 0.4641 0.0177 0.047 Uiso 1 1 calc R . .
C7 C 0.6455(4) 0.6023(4) 0.05586(17) 0.0405(10) Uani 1 1 d . . .
C8 C 0.5892(4) 0.6337(4) 0.10292(18) 0.0396(9) Uani 1 1 d . . .
H8A H 0.5807 0.7149 0.1077 0.048 Uiso 1 1 calc R . .
C9 C 0.5439(3) 0.5498(4) 0.14403(16) 0.0332(8) Uani 1 1 d . . .
C10 C 0.6418(4) 0.2735(4) 0.08270(18) 0.0447(10) Uani 1 1 d . . .
H10A H 0.6815 0.2689 0.1183 0.067 Uiso 1 1 calc R . .
H10B H 0.7017 0.2761 0.0530 0.067 Uiso 1 1 calc R . .
H10C H 0.5554 0.1941 0.0726 0.067 Uiso 1 1 calc R . .
C11 C 0.6929(5) 0.6959(5) 0.0122(2) 0.0599(13) Uani 1 1 d . . .
H11A H 0.7383 0.6627 -0.0160 0.090 Uiso 1 1 calc R . .
H11B H 0.7551 0.7866 0.0308 0.090 Uiso 1 1 calc R . .
H11C H 0.6158 0.6986 -0.0063 0.090 Uiso 1 1 calc R . .
C12 C 0.4819(4) 0.5854(4) 0.19425(18) 0.0418(9) Uani 1 1 d . . .
H12A H 0.5214 0.5731 0.2282 0.063 Uiso 1 1 calc R . .
H12B H 0.3854 0.5269 0.1901 0.063 Uiso 1 1 calc R . .
H12C H 0.4983 0.6793 0.1974 0.063 Uiso 1 1 calc R . .
C13 C 0.5010(3) 0.2008(3) 0.29825(14) 0.0262(7) Uani 1 1 d . . .
C14 C 0.6310(3) 0.2837(4) 0.33273(16) 0.0355(9) Uani 1 1 d . . .
H14A H 0.6341 0.2415 0.3653 0.053 Uiso 1 1 calc R . .
H14B H 0.6395 0.3740 0.3458 0.053 Uiso 1 1 calc R . .
H14C H 0.7047 0.2900 0.3098 0.053 Uiso 1 1 calc R . .
C15 C 0.3976(3) 0.0488(3) 0.36079(15) 0.0292(8) Uani 1 1 d . . .
C16 C 0.4084(4) -0.0713(4) 0.35855(17) 0.0362(9) Uani 1 1 d . . .
C17 C 0.3899(4) -0.1298(4) 0.40721(17) 0.0393(9) Uani 1 1 d . . .
H17A H 0.3986 -0.2103 0.4066 0.047 Uiso 1 1 calc R . .
C18 C 0.3594(4) -0.0731(4) 0.45579(18) 0.0423(10) Uani 1 1 d . . .
H18A H 0.3466 -0.1146 0.4884 0.051 Uiso 1 1 calc R . .
C19 C 0.3473(4) 0.0449(4) 0.45717(17) 0.0398(9) Uani 1 1 d . . .
H19A H 0.3261 0.0838 0.4909 0.048 Uiso 1 1 calc R . .
C20 C 0.3656(3) 0.1072(4) 0.40991(16) 0.0349(8) Uani 1 1 d . . .
C21 C 0.4350(5) -0.1373(4) 0.3052(2) 0.0555(12) Uani 1 1 d . . .
H21A H 0.4281 -0.2251 0.3102 0.083 Uiso 1 1 calc R . .
H21B H 0.5251 -0.0807 0.2953 0.083 Uiso 1 1 calc R . .
H21C H 0.3691 -0.1495 0.2749 0.083 Uiso 1 1 calc R . .
C22 C 0.3487(4) 0.2342(4) 0.41143(18) 0.0451(10) Uani 1 1 d . . .
H22A H 0.3035 0.2468 0.4447 0.068 Uiso 1 1 calc R . .
H22B H 0.2949 0.2264 0.3775 0.068 Uiso 1 1 calc R . .
H22C H 0.4367 0.3115 0.4130 0.068 Uiso 1 1 calc R . .
C23 C 0.8925(3) 0.6629(3) 0.28104(15) 0.0280(8) Uani 1 1 d . . .
C24 C 1.0795(3) 0.8673(3) 0.29821(16) 0.0331(8) Uani 1 1 d . . .
H24A H 1.1544 0.9468 0.2920 0.040 Uiso 1 1 calc R . .
C25 C 1.0380(3) 0.8326(3) 0.34798(16) 0.0350(9) Uani 1 1 d . . .
H25A H 1.0784 0.8827 0.3840 0.042 Uiso 1 1 calc R . .
C26 C 0.8584(3) 0.6350(3) 0.38036(15) 0.0293(8) Uani 1 1 d . . .
C27 C 0.9132(3) 0.5601(3) 0.40234(16) 0.0320(8) Uani 1 1 d . . .
C28 C 0.8505(4) 0.4913(4) 0.44609(16) 0.0351(8) Uani 1 1 d . . .
H28A H 0.8860 0.4394 0.4617 0.042 Uiso 1 1 calc R . .
C29 C 0.7382(4) 0.4974(4) 0.46698(15) 0.0345(8) Uani 1 1 d . . .
C30 C 0.6863(4) 0.5722(4) 0.44371(16) 0.0364(9) Uani 1 1 d . . .
H30A H 0.6084 0.5754 0.4576 0.044 Uiso 1 1 calc R . .
C31 C 0.7450(3) 0.6431(3) 0.40058(15) 0.0317(8) Uani 1 1 d . . .
C32 C 1.0333(4) 0.5503(4) 0.37943(18) 0.0437(10) Uani 1 1 d . . .
H32A H 1.1100 0.6396 0.3857 0.066 Uiso 1 1 calc R . .
H32B H 1.0147 0.5155 0.3390 0.066 Uiso 1 1 calc R . .
H32C H 1.0538 0.4894 0.3986 0.066 Uiso 1 1 calc R . .
C33 C 0.6707(4) 0.4193(4) 0.51350(17) 0.0471(10) Uani 1 1 d . . .
H33A H 0.6379 0.4721 0.5391 0.071 Uiso 1 1 calc R . .
H33B H 0.7353 0.4017 0.5344 0.071 Uiso 1 1 calc R . .
H33C H 0.5955 0.3338 0.4970 0.071 Uiso 1 1 calc R . .
C34 C 0.6855(4) 0.7234(4) 0.3749(2) 0.0484(10) Uani 1 1 d . . .
H34A H 0.7570 0.8119 0.3714 0.073 Uiso 1 1 calc R . .
H34B H 0.6203 0.7345 0.3992 0.073 Uiso 1 1 calc R . .
H34C H 0.6411 0.6755 0.3376 0.073 Uiso 1 1 calc R . .
C35 C 1.0077(3) 0.7634(3) 0.19861(15) 0.0283(8) Uani 1 1 d . . .
C36 C 0.9073(3) 0.6463(4) 0.15887(16) 0.0348(8) Uani 1 1 d . . .
H36A H 0.9308 0.6564 0.1202 0.052 Uiso 1 1 calc R . .
H36B H 0.8185 0.6421 0.1629 0.052 Uiso 1 1 calc R . .
H36C H 0.9066 0.5633 0.1674 0.052 Uiso 1 1 calc R . .
C37 C 1.1404(3) 0.8765(4) 0.12980(15) 0.0343(9) Uani 1 1 d . . .
C38 C 1.0868(4) 0.9408(4) 0.09868(17) 0.0413(10) Uani 1 1 d . . .
C39 C 1.1377(4) 0.9718(4) 0.04718(18) 0.0496(11) Uani 1 1 d . . .
H39A H 1.1042 1.0167 0.0256 0.059 Uiso 1 1 calc R . .
C40 C 1.2360(5) 0.9382(5) 0.02698(18) 0.0545(12) Uani 1 1 d . . .
H40A H 1.2695 0.9599 -0.0082 0.065 Uiso 1 1 calc R . .
C41 C 1.2850(4) 0.8731(5) 0.05819(18) 0.0511(11) Uani 1 1 d . . .
H41A H 1.3530 0.8507 0.0443 0.061 Uiso 1 1 calc R . .
C42 C 1.2370(4) 0.8396(4) 0.10937(17) 0.0415(9) Uani 1 1 d . . .
C43 C 1.2900(5) 0.7671(5) 0.1430(2) 0.0588(12) Uani 1 1 d . . .
H43A H 1.3551 0.7468 0.1221 0.088 Uiso 1 1 calc R . .
H43B H 1.2159 0.6832 0.1498 0.088 Uiso 1 1 calc R . .
H43C H 1.3334 0.8242 0.1791 0.088 Uiso 1 1 calc R . .
C44 C 0.9798(5) 0.9756(5) 0.1209(2) 0.0541(11) Uani 1 1 d . . .
H44A H 0.9023 0.8936 0.1271 0.081 Uiso 1 1 calc R . .
H44B H 0.9530 1.0181 0.0936 0.081 Uiso 1 1 calc R . .
H44C H 1.0141 1.0380 0.1566 0.081 Uiso 1 1 calc R . .
Cl7 Cl 1.02095(16) 0.44019(17) 0.05252(7) 0.0867(5) Uani 1 1 d . . .
Cl6 Cl 1.15540(15) 0.33667(18) 0.12141(6) 0.0837(5) Uani 1 1 d . . .
Cl2 Cl 1.10429(14) 0.19785(13) 0.28548(7) 0.0815(5) Uani 1 1 d . . .
Cl3 Cl 1.31198(13) 0.46936(12) 0.32612(5) 0.0626(3) Uani 1 1 d . . .
C1S C 1.1903(4) 0.3603(5) 0.2717(2) 0.0560(12) Uani 1 1 d . . .
H1SA H 1.1255 0.3963 0.2658 0.067 Uiso 1 1 calc R . .
H1SB H 1.2344 0.3581 0.2365 0.067 Uiso 1 1 calc R . .
Cl4 Cl 0.64678(17) 0.00391(14) 0.17087(9) 0.1069(7) Uani 1 1 d . . .
Cl5 Cl 0.77590(11) -0.09641(11) 0.24417(6) 0.0586(3) Uani 1 1 d . . .
C2S C 0.7647(5) 0.0445(5) 0.2259(3) 0.0661(14) Uani 1 1 d . . .
H2SA H 0.7422 0.0911 0.2591 0.079 Uiso 1 1 calc R . .
H2SB H 0.8530 0.1076 0.2155 0.079 Uiso 1 1 calc R . .
C3S C 1.0009(5) 0.3224(5) 0.0957(2) 0.0622(13) Uani 1 1 d . . .
H3SA H 0.9476 0.2310 0.0742 0.075 Uiso 1 1 calc R . .
H3SB H 0.9508 0.3349 0.1278 0.075 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0244(2) 0.0232(2) 0.0298(3) 0.00859(17) -0.00238(17) 0.00248(17)
Cl1 0.0399(5) 0.0374(5) 0.0575(7) 0.0120(5) 0.0030(4) 0.0202(4)
N1 0.0230(14) 0.0254(14) 0.0274(16) 0.0084(12) -0.0012(11) 0.0032(12)
N2 0.0246(14) 0.0244(14) 0.0256(16) 0.0069(12) 0.0003(11) 0.0048(12)
N3 0.0327(15) 0.0284(15) 0.0253(16) 0.0088(12) -0.0002(12) 0.0077(13)
N4 0.0277(14) 0.0266(15) 0.0298(17) 0.0099(13) 0.0021(12) 0.0046(12)
N5 0.0256(14) 0.0219(14) 0.0272(16) 0.0074(12) -0.0014(12) 0.0045(12)
N6 0.0306(15) 0.0270(15) 0.0328(18) 0.0101(13) 0.0005(13) 0.0026(13)
C1 0.0254(16) 0.0210(16) 0.029(2) 0.0085(14) 0.0020(14) 0.0061(14)
C2 0.0265(17) 0.0242(17) 0.031(2) 0.0086(15) -0.0038(14) -0.0028(14)
C3 0.0254(17) 0.0292(18) 0.032(2) 0.0083(16) -0.0052(15) 0.0004(15)
C4 0.0241(16) 0.0294(18) 0.027(2) 0.0117(15) -0.0027(14) 0.0048(14)
C5 0.0279(17) 0.0311(18) 0.031(2) 0.0059(15) -0.0025(15) 0.0069(15)
C6 0.0349(19) 0.043(2) 0.029(2) 0.0081(17) 0.0023(15) 0.0065(17)
C7 0.0344(19) 0.045(2) 0.033(2) 0.0201(18) -0.0026(16) 0.0058(17)
C8 0.0339(19) 0.033(2) 0.049(3) 0.0174(18) -0.0011(17) 0.0095(16)
C9 0.0275(17) 0.0309(19) 0.036(2) 0.0120(16) -0.0005(15) 0.0069(15)
C10 0.051(2) 0.041(2) 0.041(2) 0.0047(18) 0.0096(19) 0.0204(19)
C11 0.058(3) 0.065(3) 0.052(3) 0.037(2) 0.009(2) 0.016(2)
C12 0.043(2) 0.035(2) 0.049(3) 0.0107(18) 0.0118(18) 0.0168(18)
C13 0.0277(17) 0.0224(16) 0.0236(19) 0.0057(14) -0.0002(13) 0.0065(14)
C14 0.0319(18) 0.0304(19) 0.034(2) 0.0121(16) -0.0047(15) 0.0029(15)
C15 0.0237(16) 0.0280(18) 0.028(2) 0.0098(15) -0.0015(14) 0.0026(14)
C16 0.0362(19) 0.0312(19) 0.039(2) 0.0145(16) 0.0049(16) 0.0106(16)
C17 0.043(2) 0.033(2) 0.043(2) 0.0174(18) 0.0032(18) 0.0151(17)
C18 0.041(2) 0.043(2) 0.037(2) 0.0208(18) -0.0009(17) 0.0103(18)
C19 0.040(2) 0.045(2) 0.030(2) 0.0091(17) 0.0026(16) 0.0130(18)
C20 0.0318(18) 0.0336(19) 0.032(2) 0.0089(16) -0.0029(15) 0.0077(16)
C21 0.079(3) 0.045(2) 0.051(3) 0.019(2) 0.021(2) 0.033(2)
C22 0.053(2) 0.043(2) 0.040(2) 0.0065(19) 0.0032(19) 0.021(2)
C23 0.0239(16) 0.0284(18) 0.031(2) 0.0097(15) 0.0014(14) 0.0100(14)
C24 0.0268(17) 0.0233(17) 0.036(2) 0.0062(15) -0.0009(15) -0.0007(14)
C25 0.0317(18) 0.0249(18) 0.031(2) 0.0026(15) -0.0048(15) -0.0021(15)
C26 0.0307(18) 0.0235(17) 0.0269(19) 0.0080(14) -0.0006(14) 0.0050(14)
C27 0.0279(17) 0.0298(18) 0.033(2) 0.0093(15) -0.0002(15) 0.0073(15)
C28 0.0362(19) 0.0338(19) 0.032(2) 0.0082(16) -0.0059(16) 0.0123(16)
C29 0.038(2) 0.0328(19) 0.025(2) 0.0050(15) 0.0025(15) 0.0086(16)
C30 0.0353(19) 0.035(2) 0.036(2) 0.0067(17) 0.0078(16) 0.0120(16)
C31 0.0336(18) 0.0270(18) 0.030(2) 0.0040(15) 0.0010(15) 0.0100(15)
C32 0.037(2) 0.052(2) 0.048(3) 0.020(2) 0.0056(18) 0.0223(19)
C33 0.050(2) 0.051(2) 0.036(2) 0.0216(19) 0.0045(18) 0.014(2)
C34 0.053(2) 0.046(2) 0.056(3) 0.016(2) 0.008(2) 0.029(2)
C35 0.0261(17) 0.0256(17) 0.032(2) 0.0070(15) -0.0002(14) 0.0101(15)
C36 0.0327(18) 0.0298(18) 0.030(2) 0.0081(15) -0.0021(15) 0.0023(15)
C37 0.0315(18) 0.0292(18) 0.026(2) 0.0067(15) -0.0034(15) -0.0013(15)
C38 0.041(2) 0.032(2) 0.036(2) 0.0092(17) -0.0044(17) 0.0023(17)
C39 0.056(3) 0.044(2) 0.037(2) 0.0180(19) -0.006(2) 0.008(2)
C40 0.055(3) 0.056(3) 0.029(2) 0.010(2) 0.002(2) 0.004(2)
C41 0.044(2) 0.063(3) 0.036(2) 0.006(2) 0.0054(18) 0.015(2)
C42 0.036(2) 0.045(2) 0.032(2) 0.0049(18) -0.0011(16) 0.0082(18)
C43 0.059(3) 0.084(4) 0.045(3) 0.015(2) 0.003(2) 0.041(3)
C44 0.060(3) 0.061(3) 0.048(3) 0.020(2) 0.001(2) 0.029(2)
Cl7 0.0905(10) 0.0957(11) 0.0904(11) 0.0413(9) 0.0125(8) 0.0488(9)
Cl6 0.0771(9) 0.1282(13) 0.0638(9) 0.0083(8) -0.0052(7) 0.0646(9)
Cl2 0.0671(8) 0.0526(7) 0.1111(12) 0.0166(7) -0.0280(8) 0.0146(6)
Cl3 0.0714(8) 0.0520(7) 0.0543(8) 0.0099(5) -0.0078(6) 0.0185(6)
C1S 0.049(2) 0.061(3) 0.057(3) 0.016(2) -0.003(2) 0.021(2)
Cl4 0.0930(11) 0.0516(8) 0.1625(18) 0.0157(9) -0.0575(11) 0.0224(7)
Cl5 0.0560(6) 0.0450(6) 0.0782(9) 0.0191(6) 0.0146(6) 0.0229(5)
C2S 0.065(3) 0.040(2) 0.088(4) 0.009(3) -0.006(3) 0.021(2)
C3S 0.060(3) 0.066(3) 0.062(3) 0.011(3) -0.002(2) 0.029(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 C23 1.933(3) . ?
Cu1 C1 1.937(3) . ?
Cu1 Cl1 2.4313(10) . ?
N1 C1 1.350(4) . ?
N1 C3 1.399(4) . ?
N1 C4 1.441(4) . ?
N2 C1 1.379(4) . ?
N2 C2 1.401(4) . ?
N2 C13 1.431(4) . ?
N3 C13 1.266(4) . ?
N3 C15 1.420(4) . ?
N4 C23 1.355(5) . ?
N4 C25 1.394(4) . ?
N4 C26 1.435(4) . ?
N5 C23 1.385(4) . ?
N5 C24 1.398(4) . ?
N5 C35 1.427(4) . ?
N6 C35 1.259(4) . ?
N6 C37 1.429(5) . ?
C2 C3 1.328(5) . ?
C4 C5 1.398(5) . ?
C4 C9 1.399(5) . ?
C5 C6 1.388(5) . ?
C5 C10 1.516(5) . ?
C6 C7 1.393(6) . ?
C7 C8 1.381(6) . ?
C7 C11 1.527(5) . ?
C8 C9 1.408(5) . ?
C9 C12 1.494(5) . ?
C13 C14 1.493(5) . ?
C15 C20 1.399(5) . ?
C15 C16 1.401(5) . ?
C16 C17 1.398(5) . ?
C16 C21 1.492(6) . ?
C17 C18 1.371(6) . ?
C18 C19 1.388(6) . ?
C19 C20 1.391(5) . ?
C20 C22 1.516(6) . ?
C24 C25 1.339(5) . ?
C26 C27 1.393(5) . ?
C26 C31 1.398(5) . ?
C27 C28 1.405(5) . ?
C27 C32 1.500(5) . ?
C28 C29 1.384(5) . ?
C29 C30 1.384(5) . ?
C29 C33 1.521(5) . ?
C30 C31 1.391(5) . ?
C31 C34 1.523(5) . ?
C35 C36 1.491(5) . ?
C37 C42 1.389(6) . ?
C37 C38 1.403(6) . ?
C38 C39 1.397(6) . ?
C38 C44 1.496(6) . ?
C39 C40 1.383(7) . ?
C40 C41 1.379(7) . ?
C41 C42 1.386(6) . ?
C42 C43 1.509(6) . ?
Cl7 C3S 1.737(5) . ?
Cl6 C3S 1.760(5) . ?
Cl2 C1S 1.732(5) . ?
Cl3 C1S 1.761(5) . ?
Cl4 C2S 1.720(5) . ?
Cl5 C2S 1.757(5) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C23 Cu1 C1 155.34(14) . . ?
C23 Cu1 Cl1 99.29(10) . . ?
C1 Cu1 Cl1 105.35(10) . . ?
C1 N1 C3 112.6(3) . . ?
C1 N1 C4 126.0(3) . . ?
C3 N1 C4 121.4(3) . . ?
C1 N2 C2 111.1(3) . . ?
C1 N2 C13 127.4(3) . . ?
C2 N2 C13 121.5(3) . . ?
C13 N3 C15 122.6(3) . . ?
C23 N4 C25 112.3(3) . . ?
C23 N4 C26 124.6(3) . . ?
C25 N4 C26 122.9(3) . . ?
C23 N5 C24 111.6(3) . . ?
C23 N5 C35 126.5(3) . . ?
C24 N5 C35 121.9(3) . . ?
C35 N6 C37 122.5(3) . . ?
N1 C1 N2 102.9(3) . . ?
N1 C1 Cu1 123.7(2) . . ?
N2 C1 Cu1 132.9(3) . . ?
C3 C2 N2 107.0(3) . . ?
C2 C3 N1 106.4(3) . . ?
C5 C4 C9 123.1(3) . . ?
C5 C4 N1 118.3(3) . . ?
C9 C4 N1 118.6(3) . . ?
C6 C5 C4 117.7(3) . . ?
C6 C5 C10 121.5(4) . . ?
C4 C5 C10 120.8(3) . . ?
C5 C6 C7 121.6(4) . . ?
C8 C7 C6 118.8(3) . . ?
C8 C7 C11 120.7(4) . . ?
C6 C7 C11 120.4(4) . . ?
C7 C8 C9 122.5(4) . . ?
C4 C9 C8 116.2(3) . . ?
C4 C9 C12 122.4(3) . . ?
C8 C9 C12 121.4(3) . . ?
N3 C13 N2 115.3(3) . . ?
N3 C13 C14 128.1(3) . . ?
N2 C13 C14 116.6(3) . . ?
C20 C15 C16 121.0(3) . . ?
C20 C15 N3 120.2(3) . . ?
C16 C15 N3 118.2(3) . . ?
C17 C16 C15 118.3(4) . . ?
C17 C16 C21 120.8(4) . . ?
C15 C16 C21 120.8(3) . . ?
C18 C17 C16 121.3(4) . . ?
C17 C18 C19 119.8(4) . . ?
C18 C19 C20 121.0(4) . . ?
C19 C20 C15 118.6(4) . . ?
C19 C20 C22 120.6(4) . . ?
C15 C20 C22 120.8(3) . . ?
N4 C23 N5 102.8(3) . . ?
N4 C23 Cu1 124.2(2) . . ?
N5 C23 Cu1 132.5(3) . . ?
C25 C24 N5 106.3(3) . . ?
C24 C25 N4 107.1(3) . . ?
C27 C26 C31 122.1(3) . . ?
C27 C26 N4 118.0(3) . . ?
C31 C26 N4 119.9(3) . . ?
C26 C27 C28 117.7(3) . . ?
C26 C27 C32 121.4(3) . . ?
C28 C27 C32 120.9(3) . . ?
C29 C28 C27 121.6(4) . . ?
C28 C29 C30 118.9(3) . . ?
C28 C29 C33 120.3(4) . . ?
C30 C29 C33 120.7(3) . . ?
C29 C30 C31 121.8(3) . . ?
C30 C31 C26 117.9(3) . . ?
C30 C31 C34 121.2(3) . . ?
C26 C31 C34 120.9(3) . . ?
N6 C35 N5 115.7(3) . . ?
N6 C35 C36 127.3(3) . . ?
N5 C35 C36 117.0(3) . . ?
C42 C37 C38 121.5(4) . . ?
C42 C37 N6 118.7(3) . . ?
C38 C37 N6 119.4(4) . . ?
C39 C38 C37 117.7(4) . . ?
C39 C38 C44 121.9(4) . . ?
C37 C38 C44 120.4(4) . . ?
C40 C39 C38 121.3(4) . . ?
C41 C40 C39 119.6(4) . . ?
C40 C41 C42 121.2(4) . . ?
C41 C42 C37 118.7(4) . . ?
C41 C42 C43 121.0(4) . . ?
C37 C42 C43 120.3(4) . . ?
Cl2 C1S Cl3 113.3(3) . . ?
Cl4 C2S Cl5 113.0(3) . . ?
Cl7 C3S Cl6 111.9(3) . . ?
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max 1.091
_refine_diff_density_min -1.022
_refine_diff_density_rms 0.081
_vrf_PLAT601_k09221
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of . 240.00 A**3
RESPONSE: _vrf_PLAT601_k0725
During the
refinement of the structure, electron density peaks were located
that were believed to be highly disordered
solvent molecules (possibly dichloromethane and/or pentane).
Attempts made to model the solvent molecule were not successful.
The SQUEEZE option in PLATON (Spek, 2003) indicated there was a
solvent cavity of volume 240 \%A^3^ containing approximately 56
electrons. In the final cycles of refinement, this contribution to the
electron density was removed from the observed data. The
density, the F(000) value, the molecular weight and the formula are
given without taking into account the results obtained with the
SQUEEZE option PLATON (Spek, 2003). Similar treatments of disordered
solvent molecules were carried out by St\"ahler et al. (2001),
Cox et al. (2003), Mohamed et al. (2003) and Athimoolam et al. (2005).
References:
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13
Athimoolam, S., Kumar, J., Ramakrishnan, V. & Rajaram, R.K. (2005).
Acta Cryst. E61, m2014-m2017.
Cox, J.P., Kumarasammy, Y., Nahar, L., Sarkar D.S. & Shoeb, M.
(2003). Acta Cryst. E59, o975-o977.
Mohamed, A.A., Krause Bauer, A.J., Bruce, E.A. & Bruce M.R.M.
(2003). Acta Cryst. C59, m84-m86.
St\"ahler, R., N\"ather, C. & Bensch, W. (2001). Acta Cryst.
C57, 26-27.
;